Manufacture of oxalates.



F. A. DUGAN.

MANUFACTURE OF OXALATE3.

APPLICATION FILED SEPT-27,1916.

1,282,249 Patented July 3, 1917.

Fig. 1.

Inventor,

Francis A, Dug an,

AHorney FRANCIS A. JDUGAN, OF BROOKLYN, NEW YORK.

MANUFACTURE 01E OKALATES.

Specification of Letters Patent.

Patented July 3, 1%17.

Application filed September 27, 1916. Serial N 0. 122,339.

To all whom it may concern:

Be it known that l, FRANCIS A. DUGAN, a citizen of the United States of America, and a resident of the borough of Brooklyn,'in the city of New York, county of Kings, and State of New York, have invented certain new and useful Improvements in the Manufacture of Oxalates, of which the following is a specification. I

The object of this invention is to provide a process and apparatus for the expeditious manufacture of oxalates and particularly the manufacture of sodium oxalate from ,car-

bon dioxid gas and molten sodium in a.

pebble mill. To this end these two reacting materials are heated to the reaction temperature and separately introduced into the mill, the carbon dioxid forming the atmosphere of the mill-chamber and the sodium being sprayed into the chamber.

In the accompanying sheet of drawings which forms a part of this application,

Figure 1 is a vertical section through a heater and pebble mill arranged to carry out this invention.

Fig. 2 is a section through the mill on the line HIT of Fig. 1, the screen being omitted.

As shown, the carbon dioxid may be brought to the apparatus in highly compressed form in a cylinderl, from which it is admitted through a valve 2 to coils 3 3 of a heater 4: by which it is raised. to a temperature suiiicient to maintain a reaction temperature preferably of 360 G, or more where the reaction takes place. From the heater the carbon dioxid passes through a pipe 5 to a jacket '6 surrounding a tank 7. Molten sodium 8 is stored in the tank and no protected from the air by a layer of oil 9.

From the jacket a large carbon-dioxid supply pipe 10 leads to and makes a slip joint connection with a hollow trunnion 11 of a pebble mill 12. From the sodium tank contu nection is through a valve 13 located in the jacket and thence through a sodium supply pipe 14 which leads through the carbondioxid supply pipe and trunnion and terminates in a spray head 15 within the cylinder of the pebble mill. A wrapping of insulating material 16, as asbestos, covers the pipe from the heater to the tank jacket, and also the tank jacket, pipe therefrom to the mill, and the cylinder of the mill. The

cylinder is rotated by any suitable means,

as through a gear 17, and the chamber of the cylinder is partly filled with pebbles or balls 18, 18. Near one end of the cylinder is a screen 19 which divides the chamber and confines the pebbles to the lar er portion. The smaller portion of the cylinder chamber has an opening 20 from which the prod' not is delivered to a hopper 21. A con- Veyer 22 carries ofi' the product from the hopper.

In operation, the carbon dioxid on reaching the jacket of the sodium tank heats or maintains the sodium at a temperature suitable for reaction in producing the sodium oxalate and such a temperature is maintained in the carbon dioxid forming the atmosphere of the mill chamber. It is to be noted that the-carbon dioxid is initially heated to a much higher temperature to provide for the heat passing to the sodium and used up in the reaction. The molten sodium is sprayed into the carbon-dioxid atmosphere in the mill'andreacts' with the carbon dioxid to form sodium oxalate the production of which is the specific object of the process herein set forth. For the complete reaction it is necessary that all parts of the molten sodium be exposed to the carbon-dioxid atmosphere, and it has been found that the mere spraying is insufiicient. Such portions of the sodium as are not reacted upon in the spray form fall on-and spread over the large surface of the pebbles and coat them with a thin liquid film. This causes the sodium to be thoroughly exposed. The operation of the mill breaks up the resulting salt and further insures the continued exposure of the liquid sodium to the carbon-dioxid atmosphere until the. reaction is completed and all the sodium is converted into sodium oxalate. The oxalate lying between the balls becomes thoroughly pulverized after which it passes through the screen and is conveyed from the apparatus.

What I claim as new, and desire to secure by- Letters Patent of the United States, is

1. The process of manufacturingoxalates which consists in introducing. alkali metal into a pebble mill in which an atmosphere of carbon dioxid is maintained at a suflicient reaction temperature, substantially as described.

2. The process of manufacturing oxalates which consists in spraying alkali metal into a pebble mill in which an atmosphere of carbon dioxid is maintained at a sufiicient reaction temperature, substantially as described.

3. The process of manufacturing oxalates which consists in spraying alkali metal into a pebble mill in which an atmosphere of carbon dioXid is maintained at a sufiicient reaction temperature, and effecting the removal of the oxalate through a screen, substantially as described.

4. The process of manufacturing sodium oxalate which consists in introducing sodium into a pebble mill in which anatmosphere of carbon dioxid is maintained at a sufiicient reaction temperature, substantially as described.

5. The process of manufacturing sodium oxalate which consists inspraying sodium into a pebble mill in which an atmosphere of carbon dioXid is maintained at a sufiicient reaction temperature, substantially as described.

6. The process of manufacturing sodium.

oxalate which consists in spraying sodium into a pebble mill in which an atmosphere of carbon dioxid is maintained at a sufficient reaction temperature, and efiecting the removal of the sodium oxalate through a screen, substantially as described.

Signed by me at New York, NI Y., this 26th day of September, 1916.

SAMUEL W. BALOH, CHAS. F. McKnNNA. 

